反応 #1983

反応方程式

compound

1-benzyl-3-trifluoromethylpyrrolidine-3-carboxylic acid

diphenylphosphoryl azide

trimethyl amine

t-butanol

→

title compound

収率 96.7%

1-benzyl-3-(BOC-amino)-3-trifluoromethylpyrrolidine

収率 96.7%

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux under N2 for 24 hours
3. 3
   濃縮The mixture was concentrated to dryness
4. 4
   workup.DISSOLUTIONthe residue was dissolved in methylene chloride
5. 5
   洗浄The solution was washed with satd
6. 6
   濃縮NaHCO3 and water, then concentrated
7. 7
   その他The residue was chromatographed on silica gel

実験手順

A mixture of 1.42 g of the compound from step 454a, 1.71 g of diphenylphosphoryl azide, 12.3 g of t-butanol and 0.627 g of trimethyl amine was heated at reflux under N2 for 24 hours. The mixture was concentrated to dryness, and the residue was dissolved in methylene chloride. The solution was washed with satd. NaHCO3 and water, then concentrated. The residue was chromatographed on silica gel to give 1.73 g of the title compound.

出典